CN106735249A - A kind of niobium based composites and preparation method - Google Patents

A kind of niobium based composites and preparation method Download PDF

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CN106735249A
CN106735249A CN201611115516.6A CN201611115516A CN106735249A CN 106735249 A CN106735249 A CN 106735249A CN 201611115516 A CN201611115516 A CN 201611115516A CN 106735249 A CN106735249 A CN 106735249A
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based composites
powder
niobium based
preparation
ball
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CN106735249B (en
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肖来荣
余宸旭
张贝
宋宇峰
赵小军
刘建飞
郭蕾等
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Central South University
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Central South University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F2003/145Both compacting and sintering simultaneously by warm compacting, below debindering temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • B22F2007/042Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • B22F2007/042Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
    • B22F2007/045Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method accompanied by fusion or impregnation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

Abstract

A kind of niobium based composites and preparation method, belong to refractory metal base composite material preparation field.The composite is by Nb/Nb5Si3Pressure sintering is obtained after layer structure is stacked;The Nb/Nb5Si3Layer structure is made up of Nb paper tinsel surface coatings.Its preparation technology is that Nb powder and Si spheres of powder mill are prepared into slurry, and slurry is coated uniformly on into Nb paper tinsels surface, is obtained after 1500 DEG C~1750 DEG C vacuum heating-press sinterings 3 after the Nb paper tinsels after spraying/dip-coating are laminated.Rational allocation slurry compositions of the present invention, it is good with Nb paper tinsels thermal matching, form alternatively distributed Nb/Nb5Si3Layered microstructure, realizes and obtains elevated temperature strength higher in the direction parallel to layered microstructure, while obtaining the requirement of Room-Temperature Fracture Toughness higher perpendicular to the direction of layered microstructure.Product preparation process of the present invention is simple, low production cost, lamellar tissue's dense uniform, can effectively realize enhancing, toughness reinforcing and reduce the target of density.

Description

A kind of niobium based composites and preparation method
Technical field
The invention discloses a kind of niobium based composites and Nb/Nb5Si3Preparation method.One kind is particularly related to by Nb/ Nb5Si3Pressure sintering is obtained after layer structure is stacked niobium based composites and preparation method;Belong to refractory metal base composite material Preparing technical field.
Background technology
With developing rapidly for current aerospace aerospace industry, high intensity, high tenacity to high-temperature structural material, low-density are carried Demand higher is gone out.Niobium alloy be it is a kind of with high-melting-point, high intensity, high tenacity excellent structural material, extensively should It is especially extremely wide in the application of aerospace craft for fields such as Aero-Space.It is high using addition more than existing niobium alloy Melting point metals element carries out solution strengthening, and while intensity is improved, density is consequently increased.According to addition element species and contain The difference of amount, the temperature in use scope of niobium alloy is generally 1100~1400 DEG C, and elevated temperature strength is generally 150~300MPa, close Degree scope is 8.6~11g/cm3
At present, the main direction of studying of high-strength light niobium based composites is Nb-Si based materials.U.S. Lai Te laboratories, Lao Lunsilifu moles of National Laboratory, Surrey university, Tokyo University of Science and Technology, domestic Shanghai Communications University, western Beijing Polytechnical University, Large quantities of scientific research institutions such as Central South University have carried out the relevant research work of Nb-Si composite materials.Existing Nb-Si systems are multiple Condensation material, generally prepares casting using founding, then, casting is heat-treated, and obtains with Nb5Si3For main high temperature is strong Change the Nb-Si composite materials of phase, as the niobium based solid solution Nb of Plastic phasessRoom-Temperature Fracture Toughness, but this kind of material are then provided Still it is primarily present problems with:(1) material Room-Temperature Fracture Toughness still is apparent not enough.It is combined by the Nb-Si systems after founding, heat treatment Material, in NbssAnd Nb5Si3In the case of respectively accounting for 50% volume fraction, Room-Temperature Fracture Toughness only 6.5MPam1/2, greatly limit The application of material is made.(2) the Nb-Si composite materials after founding, hardening constituent is Nb3Si, this mutually be metastable phase, it is necessary to Less than 1770 DEG C heat treatment more than 100h can be completely decomposed into Nb5Si3So that material flow in preparation process increases, effect Rate reduction.Due to the presence of these problems, the practical application of Nb-Si composite materials is greatly constrained, while also limit me The development of state's space flight and aviation level.
The content of the invention
It is an object of the invention to the problem for overcoming existing niobium based composites to exist, there is provided a kind of preparation process is simple, Cost is relatively low, intensity and fracture toughness niobium based composites higher and preparation technology, solves the fracture of niobium based composites room temperature The relatively low problem of toughness.
A kind of niobium based composites of the present invention, the niobium based composites are by Nb/Nb5Si3Pressure burns after layer structure is stacked Knot is obtained;The Nb/Nb5Si3Layer structure is made up of Nb paper tinsel surface coatings, the coating by mass percentage, including under State component:
Nb powder 50%~90%, Si powder 10%~50%.
A kind of niobium based composites of the present invention, the Nb paper tinsels thickness is 15~35 μm, and the purity of Nb paper tinsels is more than or equal to 99.9%.
A kind of niobium based composites of the present invention, the average particle diameter size of Nb powder is 1~5 μm, the average particle diameter size of Si powder It is 1~5 μm;Nb powder, the purity of Si powder are all higher than being equal to 99.9%.
A kind of niobium based composites of the present invention, the coating layer thickness is 10 μm~80 μm.
A kind of preparation method of niobium based composites of the present invention, comprises the steps:
After step one, Nb paper tinsels are processed through pickling, alkali cleaning, ultrasonic wave is cleaned up in alcohol, drying;
Step 2, the quality proportioning by design, taking during Nb powder, Si powder are put into ball grinder carries out wet ball grinding, obtains slurry;
Step 3, gained slurry in step 2 is evenly applied to the Nb paper tinsels surface that is obtained in step one, after drying;To be many Layer Nb paper tinsels are stacked, under vacuum condition, be warming up to 1500 DEG C~1750 DEG C carry out pressure sintering after lower the temperature with stove, obtain niobium base and be combined Material.
A kind of preparation method of niobium based composites of the present invention, in step 2, the ball-milling medium of wet ball grinding is quality hundred Divide ethanol solution of the concentration more than or equal to 99.9%, ball-milling medium consumption is 1.5~3.5 times of ball milling quality of material, ball material matter Amount is than being 3:1~10:1;Ball-milling Time 10h~15h, drum's speed of rotation is 200r/min~400r/min.
A kind of preparation method of niobium based composites of the present invention, in step 3, slurry is uniform by the way of spraying/dip-coating Nb paper tinsels surface is coated on, the feed pulp layer that thickness is 10 μm~80 μm is formed;Heating rate is 5~10 DEG C/min, during sintered heat insulating Between be 30min~100min, furnace pressure be 40~60Mpa, in stove vacuum be less than or equal to 0.01Pa.
A kind of preparation method of niobium based composites of the present invention, the niobium based composites of preparation, 1400 DEG C of compression strength It is 200-400Mpa;Fracture toughness is 15-20MPam at room temperature1/2;Room temperature lower density is 7.8~8.0g/cm3
Principle and advantage:
The present invention is main body formula with Nb paper tinsels, Nb powder and Si powder, coats what Nb powder and Si powder were constituted by Nb paper tinsels surface , there is reaction in-situ generation Nb then during hot pressed sintering, between Nb powder and Si powder, Si powder and Nb paper tinsels in slurry5Si3Phase, Nb There is diffusion reaction between powder and Nb paper tinsels, while under the effect of the pressure, hole disappears between each phase, material is densified, Nb layers and Nb5Si3Presentation is alternately distributed, and promotes the lifting of the elevated temperature strength and Room-Temperature Fracture Toughness of material.
Composite of the invention is main that following reaction occurs during hot pressed sintering:
Nb+Si=Nb5Si3 (1)
Nb will be with Si reaction generations Nb under high temperature5Si3, because sintering temperature control is in Nb3Si-Nb5Si3Solid phase transition temperature Hereinafter, metastable Nb is there will not be in sintering process3Si phases so that material is without follow-up long-time high-temperature heat treatment, contracting Short technological process.
Alternatively distributed NbssLayer and Nb5Si3The elevated temperature strength of the composite is improved, mainly due to following two originals Cause:(1) elevated temperature strength of material mainly determines by the volume fraction of hardening constituent, the present invention by controlling the thickness of coating, and then Realize the hardening constituent Nb of control composite5Si3Volume fraction reaches 30%~80%, material is had elevated temperature strength higher; (2) distribution form of the elevated temperature strength of material also with hardening constituent is relevant, and the present invention is used hardening constituent Nb5Si3In the composite In layered distribution, parallel to Nb5Si3On the direction of layer, intensity has further raising.
Alternatively distributed NbssLayer and Nb5Si3The Room-Temperature Fracture Toughness of the composite is improved, mainly due to following two Individual reason:(1) Room-Temperature Fracture Toughness of material is influenceed larger by the distribution form of Plastic phase.The Plastic phase of composite of the present invention NbssIn layered distribution, perpendicular to NbssOn the direction of layer, Crack Extension needs the Nb through plasticity all the timess, through Nbss When, crackle there occurs the behaviors such as deflection, bifurcated and bridge joint, consume big energy, make the Room-Temperature Fracture Toughness of material notable Increase.(2) size of the Room-Temperature Fracture Toughness of material also with Plastic phase is relevant, and size is bigger, and Room-Temperature Fracture Toughness is higher.This hair The bright Nb by controlling material plasticityssThe average-size of phase makes Room-Temperature Fracture Toughness further improve at 15~35 μm.
The present invention prepares niobium based composites using spraying/dip-coating+hot pressing sintering method.Compared with the existing methods, this hair Bright preparation process is simple, production cost is relatively low, and the material prepared has elevated temperature strength and Room-Temperature Fracture Toughness higher, 1400 DEG C of intensity reaches 200-400Mpa, and more than 50% is increased compared with prior art, and Room-Temperature Fracture Toughness reaches 15-20MPa m1/2, increasing by more than 100% compared with prior art, density is 7.8~8g/cm3, it is suitable with prior art.
Brief description of the drawings:
Accompanying drawing 1 is the XRD diffraction spectras of niobium based composites;
Accompanying drawing 2 is the cross-sectional morphology of niobium based composites;
As can be seen from Figure 1:Nb is only existed after the Composite SinteringssAnd Nb5Si3Two-phase, has no Nb3Si phases are generated, nothing Long-time high-temperature heat treatment need to be carried out.
As can be seen from Figure 2:Nb layers of the composite is alternately distributed with feed pulp layer in stratiform, is conducive to the high temperature of material The lifting of intensity and Room-Temperature Fracture Toughness.
Specific embodiment:
The present invention is described in further detail with reference to the accompanying drawings and examples.
Comparative example:
Electric arc melting prepares Nb-16Si (at.%) alloy:Nb, Mo and Si simple substance of purity more than 99.9%, electric arc melting After be heat-treated, Technology for Heating Processing be 1700 DEG C be incubated 48 hours.The alloy is 190Mpa in 1400 DEG C of intensity, and room temperature is broken Toughness is split for 7MPam1/2, density is 8.1/cm3
Embodiment 1
(1) Nb paper tinsels pretreatment:Nb paper tinsels are carried out into pickling, alkali cleaning treatment, acid solution composition is HCl:HNO3:H2O=1:3:16 (volume fraction), alkali lye composition is the NaOH solution that pH value is 13, and then ultrasonic wave is cleaned up in alcohol, drying.
(2) prepared by slurry:By the Nb powders that granularity is 1 μm and the Si powders that granularity is 1 μm Nb by mass percentage 80%th, Si 20% (above material purity is not less than 99.9%), it is put into ball grinder, with ethanol solution as dispersant, hard Alloying pellet is abrading-ball, and wet ball grinding 10h obtains slurry;Alcohol consumption is ball milling quality of material (total matter of Nb powders and Si powders Amount) 1.5 times, ratio of grinding media to material is 3:1, rotating speed is 200r/min.
(3) it is uniform to coat slurry and dry:Slurry described in (1) is evenly applied to the Nb paper tinsel tables that average thickness is 20 μm Face, the feed pulp layer that thickness is 10 μm is formed on surface, then by the Nb paper tinsels drying of surface coating feed pulp layer.
(4) vacuum heating-press sintering:It is put into vacuum sintering funace after the Nb paper tinsels of drying in (2) are laminated, is evacuated to Vacuum is, less than or equal to 0.01Pa, 1500 DEG C to be warming up to the heating rate of 10 DEG C/min, applies pressure 40MPa, insulation 30min, after furnace cooling take out, formed have be alternately distributed Nb/Nb5Si3Layer structure tissue, material XRD diffraction spectras after sintering With cross-sectional morphology respectively as shown in accompanying drawing 1, Fig. 2.
(5) niobium based composites dense structure prepared by embodiment, no significant defect.Niobium base manufactured in the present embodiment is answered Condensation material Nb/Nb5Si3High temperature compressed experiment is carried out at 1400 DEG C, its compression strength is 200MPa.Resisted using 3 points at room temperature Curved method carries out fracture toughness test, and its fracture toughness is 20MPam1/2, density is 8.0g/cm3
Embodiment 2
(1) Nb paper tinsels pretreatment:Nb paper tinsels are carried out into pickling, alkali cleaning treatment, acid solution composition is HCl:HNO3:H2O=1:3:16 (volume fraction), alkali lye composition is the NaOH solution that pH value is 13, and then ultrasonic wave is cleaned up in alcohol, drying.
(2) prepared by slurry:By the Nb powders that granularity is 3 μm and the Si powders that granularity is 1 μm Nb by mass percentage 85%th, Si 15% (above material purity is not less than 99.9%), it is put into ball grinder, with ethanol solution as dispersant, hard Alloying pellet is abrading-ball, and wet ball grinding 12h obtains slurry;Alcohol consumption is ball milling quality of material (total matter of Nb powders and Si powders Amount) 2.5 times, ratio of grinding media to material is 6:1, rotating speed is 300r/min.
(3) it is uniform to coat slurry and dry:Slurry described in (1) is evenly applied to the Nb paper tinsel tables that average thickness is 25 μm Face, the feed pulp layer that thickness is 50 μm is formed on surface, then by the Nb paper tinsels drying of surface coating feed pulp layer.
(4) vacuum heating-press sintering:It is put into vacuum sintering funace after the Nb paper tinsels of drying in (2) are laminated, is evacuated to Vacuum is, less than or equal to 0.01Pa, 1650 DEG C to be warming up to the heating rate of 10 DEG C/min, applies pressure 50MPa, insulation 70min, after furnace cooling take out, formed have be alternately distributed Nb/Nb5Si3Layer structure tissue.
(5) niobium based composites dense structure prepared by embodiment, no significant defect.Niobium base manufactured in the present embodiment is answered Condensation material Nb/Nb5Si3High temperature compressed experiment is carried out at 1400 DEG C, its compression strength is 320MPa.Resisted using 3 points at room temperature Curved method carries out fracture toughness test, and its fracture toughness is 17MPam1/2, density is 7.9g/cm3
Embodiment 3
(1) Nb paper tinsels pretreatment:Nb paper tinsels are carried out into pickling, alkali cleaning treatment, acid solution composition is HCl:HNO3:H2O=1:3:16 (volume fraction), alkali lye composition is the NaOH solution that pH value is 13, and then ultrasonic wave is cleaned up in alcohol, drying.
(2) prepared by slurry:By the Nb powders that granularity is 5 μm and the Si powders that granularity is 1 μm Nb by mass percentage 90%th, Si 10% (above material purity is not less than 99.9%), it is put into ball grinder, with ethanol solution as dispersant, hard Alloying pellet is abrading-ball, and wet ball grinding 15h obtains slurry;Alcohol consumption is ball milling quality of material (total matter of Nb powders and Si powders Amount) 3.5 times, ratio of grinding media to material is 10:1, rotating speed is 400r/min.
(3) it is uniform to coat slurry and dry:Slurry described in (1) is evenly applied to the Nb paper tinsel tables that average thickness is 30 μm Face, the feed pulp layer that thickness is 80 μm is formed on surface, then by the Nb paper tinsels drying of surface coating feed pulp layer.
(4) vacuum heating-press sintering:It is put into vacuum sintering funace after the Nb paper tinsels of drying in (2) are laminated, is evacuated to Vacuum is, less than or equal to 0.01Pa, 1750 DEG C to be warming up to the heating rate of 10 DEG C/min, applies pressure 60MPa, insulation 100min, after furnace cooling take out, formed have be alternately distributed Nb/Nb5Si3Layer structure tissue.
(5) niobium based composites dense structure prepared by embodiment, no significant defect.Niobium base manufactured in the present embodiment is answered Condensation material Nb/Nb5Si3High temperature compressed experiment is carried out at 1400 DEG C, its compression strength is 400MPa.Resisted using 3 points at room temperature Curved method carries out fracture toughness test, and its fracture toughness is 15MPam1/2, density is 7.8g/cm3
Compared with comparative example, the niobium based composites prepared in embodiment in the case where density is not increased, with being higher by 50% elevated temperature strength and the Room-Temperature Fracture Toughness for being higher by 100%, greatly improve the mechanical property of material.Additionally, embodiment The material of middle preparation reduces energy ezpenditure, the production efficiency of raising without prolonged high-temperature heat treatment.
The above, only presently preferred embodiments of the present invention, therefore can not according to this limit the scope of present invention implementation, i.e., The equivalence changes made according to the scope of the claims of the present invention and description and modification, all should still belong in the range of the present invention covers.

Claims (10)

1. a kind of niobium based composites, the niobium based composites are by Nb/Nb5Si3Pressure sintering is obtained after layer structure is stacked; The Nb/Nb5Si3Layer structure is made up of Nb paper tinsel surface coatings, the coating by mass percentage, including following components:
Nb powder 50%~90%, Si powder 10%~50%.
2. a kind of niobium based composites according to claim 1, it is characterised in that:The Nb paper tinsels thickness is 15~35 μm, The purity of Nb paper tinsels is more than or equal to 99.9%.
3. a kind of niobium based composites according to claim 1, it is characterised in that:The average particle diameter size of Nb powder is 1~5 μm, the average particle diameter size of Si powder is 1~5 μm;Nb powder, the purity of Si powder are all higher than being equal to 99.9%.
4. a kind of niobium based composites according to claim 1-3 any one, it is characterised in that:The coating layer thickness is 10 μm~80 μm.
5. a kind of preparation method of niobium based composites as claimed in claim 4, comprises the steps:
After step one, Nb paper tinsels are processed through pickling, alkali cleaning, ultrasonic wave is cleaned up in alcohol, drying;
Step 2, the quality proportioning by design, taking during Nb powder, Si powder are put into ball grinder carries out wet ball grinding, obtains slurry;
Step 3, gained slurry in step 2 is evenly applied to the Nb paper tinsels surface that is obtained in step one, after drying;By multilayer Nb Paper tinsel is stacked, and under vacuum condition, being warming up to 1500 DEG C~1750 DEG C lower the temperature with stove after pressure sintering, obtains niobium base composite wood Material.
6. the preparation method of a kind of niobium based composites according to claim 5, it is characterised in that:In step 2, wet method The ball-milling medium of ball milling is ethanol solution of the mass percentage concentration more than or equal to 99.9%, and ball-milling medium consumption is ball milling material matter 1.5~3.5 times of amount, ball material mass ratio is 3:1~10:1.
7. the preparation method of a kind of niobium based composites according to claim 6, it is characterised in that:Ball-milling Time 10h~ 15h, drum's speed of rotation is 200r/min~400r/min.
8. the preparation method of a kind of niobium based composites according to claim 5, it is characterised in that:In step 3, slurry Nb paper tinsels surface is evenly applied to by the way of spraying/dip-coating, the feed pulp layer that thickness is 10 μm~80 μm is formed.
9. the preparation method of a kind of niobium based composites according to claim 5, it is characterised in that:In step 3, heat up Speed is 5~10 DEG C/min, and the sintered heat insulating time is 30min~100min, and furnace pressure is 40~60Mpa, vacuum in stove Less than or equal to 0.01Pa.
10. the preparation method of a kind of niobium based composites according to claim 5, it is characterised in that:1400 DEG C of resistance to compression Intensity is 200-400Mpa;Fracture toughness is 15-20MPam at room temperature1/2;Room temperature lower density is 7.8~8.0g/cm3
CN201611115516.6A 2016-12-07 2016-12-07 A kind of niobium based composites and preparation method Expired - Fee Related CN106735249B (en)

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CN107900352A (en) * 2017-12-19 2018-04-13 哈尔滨理工大学 A kind of stratiform high niobium containing titanium aluminium alloy composite panel and preparation method thereof
CN108085526A (en) * 2017-12-15 2018-05-29 中南大学 A kind of low-density niobium based composites and preparation method
CN108411136A (en) * 2018-03-30 2018-08-17 陕西理工大学 SiGeC three niobiums enhancing Nb based high-temperature alloys of one kind and preparation method thereof
CN110193601A (en) * 2019-06-13 2019-09-03 金堆城钼业股份有限公司 A kind of preparation method of bilayer or multilayer refractory metal composite pipe
CN112276330A (en) * 2020-11-06 2021-01-29 西北工业大学 Niobium-silicon intermetallic compound composite material, preparation method thereof and diffusion welding die

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102744928A (en) * 2012-07-25 2012-10-24 哈尔滨工业大学 Preparation method for Ti3Al-TiAl laminated composite material
CN103264542A (en) * 2013-05-14 2013-08-28 哈尔滨工业大学 Titanium aluminum-ceramic layered material and preparation method thereof
WO2015166831A1 (en) * 2014-04-28 2015-11-05 国立研究開発法人宇宙航空研究開発機構 Heat-resistant metal member, method for producing heat-resistant metal member, alloy coating film, method for producing alloy coating film, rocket engine, artificial satellite and gas turbine for power generation

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102744928A (en) * 2012-07-25 2012-10-24 哈尔滨工业大学 Preparation method for Ti3Al-TiAl laminated composite material
CN103264542A (en) * 2013-05-14 2013-08-28 哈尔滨工业大学 Titanium aluminum-ceramic layered material and preparation method thereof
WO2015166831A1 (en) * 2014-04-28 2015-11-05 国立研究開発法人宇宙航空研究開発機構 Heat-resistant metal member, method for producing heat-resistant metal member, alloy coating film, method for producing alloy coating film, rocket engine, artificial satellite and gas turbine for power generation

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《ACTA METALL.MATER.》 *
《航空材料学报》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107365934A (en) * 2017-07-27 2017-11-21 中南大学 A kind of SiCp/ Cu copper foil lamination composites and preparation method thereof
CN108085526A (en) * 2017-12-15 2018-05-29 中南大学 A kind of low-density niobium based composites and preparation method
CN107900352A (en) * 2017-12-19 2018-04-13 哈尔滨理工大学 A kind of stratiform high niobium containing titanium aluminium alloy composite panel and preparation method thereof
CN108411136A (en) * 2018-03-30 2018-08-17 陕西理工大学 SiGeC three niobiums enhancing Nb based high-temperature alloys of one kind and preparation method thereof
CN110193601A (en) * 2019-06-13 2019-09-03 金堆城钼业股份有限公司 A kind of preparation method of bilayer or multilayer refractory metal composite pipe
CN112276330A (en) * 2020-11-06 2021-01-29 西北工业大学 Niobium-silicon intermetallic compound composite material, preparation method thereof and diffusion welding die

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